Bkhan3

Yes, that is the catalyst of choice here - can also use basic copper carbonate and I had some. I have to make some of the other which I will do and try this again. Thanks.

Sorry, you're not talking about metal salts, my bad. For metal hydrates, you just need to use the correct molar mass (the anhydrous form and the hydrated forms have different molar masses) when weighing amounts. For example, if you are weighing 0.1 mole of anhydrous CuSO4 use its molar mass (0.1 mol x 159.60 gmol-1 = 15.96 g). If you are weighing 0.1 mole of the pentahydrate (0.1 mol x 249.69 gmol-1 = 24.97 g). They both contain the same amount of copper.

The usual way seems to be heating a mix of Niacin and catalyst (I used basic copper carbonate) and limiting temp at the heating mantle to 250 deg C. I put a K-type thermocouple between the mantle and distillation flask. After 2 hours the head temp was only 60 deg C and nothing was happening (actually something was happening the Niacin was melting with drops forming in the head). So I raised the mantle temp and started getting distillate. Problem is the Niacin sublimes as a white vapor passing over to the receive flask, the Niacin in the rxn flask is burning and recrystallizing in the rxn flask. A loss of yield. Do I have to just let it sit at 250 deg C mantle temp?

Use 0.1 mol of the other metal compound that will react with the 0.1 mol copper sulfate solution for a stoichiometric double displacement rxn (as long as both starting reagents are 1:1 in the balanced equation). EDIT: Just do what you did for the copper sulfate solution for the other metal compound: "If I make up a 0.1 molar solution of copper sulfate at 100ml volume I need 2.49g of copper sulfate in 100ml water. "